Process for producing absolute alcohol



l. CLAPP4 PROCESS FOR PRODUGING ABSOLUTE ALCOHOL Fe'b. 19, 1929.

Filed May 18, 1925 2 Sheets-Sheet 2 MSN m &

@N uw.

SSS@ www@ Patented eb. 19, i929.

UNTE STATES PATENT OFFICE.

ELWOOD I. OLAP?, OF BALTIMORE, MARYLAND. ASSIGNOR TO U'. S. INDUSTRIALALGO- HOL CO., A CORPORATION OF VEST VIRGINIA.

PROCESS 'FOR PRODUCING ABSOLUTE ALCOHOL.

Application filed May 18, 1925.

y invent-ion relates to the production of absolute alcohol in anadvantageous manner, from alcohol ot comparatively low strength.

rllhe object otl my invention is to provide a process whereby absolutealcohol may be obtained from alcohol having a low strength and which hasmany advantages over previous proces es provided tor this purpose. 'l'he object ot' my invention is ifiarticularly to provide a. continuousprocess t'or the production otl absolute alcohol trom beer. illy presentprocess contains. amore` others. the following important features. lnthe course of my process the alcohol is Yted while hot into thedehydrating column, thus eliminating` the cost ot supplying steam toheat the liquid up to the temperature at. which it is ted into thedehydrating column. ln accomplishing this, my process comprises, ingeneral. a beer still treatment trom which the alcohol ot approximately95% strength is i'ed directly into the dehydratingl column, thuseliminating' the column previously used, as set forth in my applicationupon. absolute alcohol process. Serial No. 750,519, filed November 18,1924, for bringing' the dilute alcohol obtained from the constantboiling mixture evolved at the top ot the dehydratinp; colun'm up to 05%strength. In addition, my process comprises the treatment ot the l'useloil obtained from the beer still so as to remove ethyl alcohol and Watertherefrom and deliver a Washed fusel oil capable ot being utilized aseoinn'icrcial fuse-l oil. One feature of the 'insel oil treatment torecover the alcohol obtained in WashingY the fusel oil and to return allthe alcohol obtained in the fusel oil treatment back to the beer still.rThere also a saving' in avoiding' at this point, an;V separatedistillation ot the alcohol from the 'la el oil treatment. This tuseloil treatment is a distinct ad vantage as compared with the operationoit the process as set it'orth in in): application upon process ttor thedistillation ot alcohol. Serial No. 1.597, tiled January l0. i925. Also,another feature of my process is, if desired, to return the dilutealcohol obtained in the separation chamber connected to the dehydrationcolumn, to the insel oil column instead of to the beer still, thusobtaining' a more concentrated slop from the bottom ot the beer still.Still another feature ot importance in my process is the redistillaticnot' the absolute alcohol so as to remove any foreign materials, such asdirt or Serial No. 30,926.

other solid matter that may accumulato in the alcohol while passingthrough the process. By carrying out the process continuously in this aythere is, in general. a decided saving', also, because of the avoidanceof the use of extensive storage tanks that would be necessary it theprocess were carried out otherwise. Furthermore. the product isparticularly pure owing to the removal of the foreign solid materialstherefrom. In general. a. hotter control oit the entire process isobtainable and at a lower cost ol. operation, and a more uniformproduct, both in the case of the absolute alcohol and commercial useloil, is obtained.

l11 urther objects ot my invention will appear lrom the description ofthe same hereinafter in detail.

lYhile my invention is capable of being carried out in connection withmany different types of apparatus, bywvay ot illustration l have shownonly certain types of apparatus lor use in connection therewith, in theaccompanying drawings, in Which- Fig. l is a diagran'nnatic view of anapparatus tor use in connection with my invention, and

Fig'. 2 is a modification of the same.

For example, in carrying' out my invention l may supply beer containingapproximately 5 to 10% by volume of ethyl alcohol. through a pipe l to adcphleemator 2 from which the beer passes b v a trapped pipe 3 to a beerstill el. The beer still Llmay be heated with live steam suppliedthrough a pipe 5, or may. instead` be provided with the usual type ofheater for supplying' indirect heat such as is used in connection withan alcohol still. The slop, substantially 'free from alcohol, from thcbeer still passes out by means ot a trapped pipe G which may, ifdesired, pass through a prehcatcr T through which the pipe 3 may be madeto pass, as shown in Fig. 2 in the drawings. The vapors from the beerstill Il pass out ot the column by means ot a pipe S to the dephlcgmator2, said vapors havingbeen 0btained by reason ot' the countercurrent ofsteam in the beer still 4rtlowing upwardly against the descending,-current of liquid. Slightly above the beer inlet ot the pipe 3 there isprovide-d a thermometer 9 so as to maintain the temperature at this partof the column at approximately 89 C. so as to ohtain alcohol vaporshaving a strength of 95 to 96%, alter passing through the upper part ofthe column 1 1-, which zielig as :2. recifiijiiig i?, willich isconnececl it@ fue. beur still. unit. The high boiling impm'igiescc'aimu- "`iii "'li /l "no tl LOD Gti' 'lille licei' Still lievi 'he V;DOES late to tlii' greatest' stiengli slightly 'i the beer inist 3 and,zwcmiilingly. :i il d trapped pipe l is pimfidefl, llav 'blume Czzlvealcomwcions 1L 12 and 13 lo Liiioiii plates in the licei* still :it thiswirt ci the saune. The pipa l() lsuls to a fus .l m 14 ai; a pointSulilatzmtially 520 Dizier' bottom of tlm Same, Smil Collin fi i L sul@from the ciQ} )lileiii i izo the siifoi'l f 'empem'luire 8S@ C.,inasmuch as any top of they columa 14. by means; Gl' a. mippsd. rise inthe mupei'z ture s Couneiased by ing pipe md :i mit of the Conflmifis@gfiiinefl @Teaming the iufiuuiit oil in 'lle coiilensaii' also passaisiJ1\.C` l@ d1@ lop top @if die Column 3U of lia :Uliimn thi'ougli a pig@26, which is 'Elia @duf-mn il?) i5; hewn, .f1 fi. stamm coil 95cominctnfl lo ills pigs 2. The, imifiiiimlsy of il und cmiequsiily.lili@ :il Ji" es and @ber The Coi densi-:ite 0ll alcohol :from the@muienssei' 1 1 ai i., :1s al- Q isi lied b i a pipe 27 having :1ivnlve,915%. t0 ;.M :mi o lili@ column l'ii'ouffli a V the clliyflrnting ColumnL10 be lieieilaii'tfzl' 76- 39 a (lepliii-gn :filiir 53 @Coleiwi; cii'edto. lli mda? to main ain the liuscl cil Current of 'Willey by meins; ofinlet and ou" it 10U fuif'l 58. l

)prmih dfenscil Ysipi ;V Y 40 i'imtoljv Si@ C. zii' his nomi; m itl acolumn m a cfiiiilimwci: Si minimi Y. ,l :i @u1-lvmm cold 105 j 0'? il.inici pipe ($2 :il am 'flic l :ed @me fili taining some alcohol. back t0th conne-fried lo lli@ pipe 70 so as to convey he h5 umn -l. The fuselOil obizlinfli Q lffiiliol om lli@ Condenan.' 22 to i'zli illiy-vsuliciently high grade ifa be drilling; izolumu 72. In ordm' toclelijflmm Cmd@ 'usel oil but can, if (lesii s A. ill/1e alcohol in theColumn T? with time .fiifl of pmiierfl by distillation and reu icmii. alliii'fl liquid. any dsiied Illini liquidi maf-y' G5 The condensateobtained iii "Ellecleplileg be need foithis purpose 'which oims i Qii.-130 Slant hoiling' mixture with lhe alcohol hav- 'ng av lower hoilingpoint l'han lhe alcohol ind the n'aer preaenl'` 'hereiin hut 'For ihin`purpose l prefer l i uae henaoh fiiaerdinglv. seilieienl' henzol isaupplied lo i'he column 7:? 'l'roin a heuzol tank T?, having' a pipeif-l provided with a valve T5 `which is eoimecled to a Vliapped pipe Tocalling` to lhe side oif the column 72.

li, will he noled lhal lhe lienzol einenl the column T2 ai he same plaieas in llie ease of the pipe TO conveying the aleohol thereto. lfdeairelh also. it will he iinilerrajood lha"A lhe alcohol and beni/,olma)Y he mixed togel'her previoun4 lo eonveving l'he same ino lhc eolumnnv euilgahle healer for lhe lower end ol the column T may he uned hulY'lfor ihis purpose l have provided a Steam eoil TT and lhe amount` of insupplied lo ihe healer niav hc i fiala in aug.' suialile manner enmainl'ain n au'lieienl presaure therein. lllhen condilionpl ofefplilihrium are ohlaineel in Jdie column 72, a eonatanl' hailingAlernary mixture eoinprisiue' approxiniaieljv, h v weighlliSfb ethylalcohol J henzol will he evolved from the sop oil lhe eoluinn T2ihrougjh a pipe T8. ln order lo lQeeure these operaliug' conditions alhermomeer TS) i:-: provided in the column lo maia'iain at this point aleinperalure el approiiimal'el\v 790 C. A* this peint the alcoholcontains,` a sligh race of lienzol. lf 'lhe l'emperahire there increasesilove thin l'einperalure, this4 would he an indication ol lhe hialiageel' benz/,ol or .loss of lhe henfiol in 'he vash wal'er or incompleteremoval ol" the same from lhe alcohol, and, aoiordiug'lvsome il'url'hin'hen Zol Vwould then he added irom i'he lanh G12 lo supply i'he losa.lhni'lurinore. in ehlainiuey the cone-faul lioilinni lei-nary mixlure aiihe iop ol' he foliunu il ia dei rihle lo ohiaiu a le npral'ure alii'hal porl'ion olf he apparai lua4 of ainkn'oximalelv (35's ll.. alhermomel'er lil heilig' provided for lhal purpose. 'lhe numher olEplates in the column i2, ahove the pipe4 To and Til. should hesullieieul io produee he conslani boiling' leraar;v mivl'ure al' he iopplaie, The vapor-a l'i ui lha eolunui 'T15 which pas# out lhreuih i ,epipe 'iii are conveyed lo a dephlelmaor al. cooled will: a currenr olvaler h v inean l ol' au inleli pipe Si?l and an oullel; pipe m r"heeonilenwale is o .o ,all (lin uw. l rei'urned hy a pipe S-l lo the topoz the column 'T2 as a reflux and the uneondensed vapors f through apipe S3 lo a condenser 86, cooled `with a current ol water hy means ofan inle'l pipe Si' and an outletpipe SS, where the vapors are condenaedand cooled. The current of vvaer supplied lo the dephleglnalor Sl andlie eendenaer 86 mayv he eonlrolhid in anyv ssuiiahle way.

The condensaie paSseS our by a pipe S9 having; a. vent 9() and pari ellhe ondeusaie ia reiurned by a l apped pipe 0 l lo the pipe 8l to herel'urned lo l'he column 72. 'lhe porl'iou returned hy 'he pipe 91 iscontrolled h v a valve 92 in an outlet` pipo 93 'for l'he main pori'ionol' the condensate, which eouvev.`l lhe Aaaiue lo a separalinp' ehamherQ-l where l'he liquid separates inl'o two layers. 'l'h-e op layercontaining' principally henzol comprise` approximately hy volume` 86.5%he; :col

3.221? alcohol and .3% waier. while lhe lower layer. containing moal'llynpleousalcohol, eomilirises approximately7 ,1v volume- 'lljlfa henzol."SGfl-'fi alcohol and 32.5% valer. rl`he upper. or henzol laver. passe4oul'` ol lhe oeparaline chamber 9-1 lo the vened trapped pipe To. ll:desired, howeven 'he pipe 7G. in-

ad o l" enlering the column 'T2 dire/elly, may he eonneeled lo llhedilute, alcohol inlet pipe 'T0 hv nieanr1 or' a pipe 7G, as shown inFig. 2, so lhai the henscol. alcohol and the he i'flol and alcoholohiained 'from the ternary mixture, maj,v he mixed outside oil' hecolumn helfore eni'erinej ihe Sanne. The hol'loin laver passes oul: o?l'he separator 94; by means olli a vented pipe 95 which arranged to actas i level regulating; devil-e, and thence, lo a seruhher 9G where iheliquid is washed by means; of waler 'led ioo lthe saine lhroi'inh a pipe9T. This' reaulls in lhe 'fornialion of two liquid layers in he scruhher9G` the upper laver conlaining' eulmltantially all oi' the henzolremainingI in he liquid, and comprising approxiinalely, hy volume--Sllifj/a henzol /Tf alcohol and (LOC/a wafer and l'his upper layer if:conveyed hl" a l'rapped pipe, 9S lo i'he pipe 76 and thence hack lo illecolumn In this wav suhsantially all oi Jche benz/iol is returned lo heused ove again in the process. .ln the scrubber fhe lower laver,eomprisiueY wash water, and Containing); hy volunic- 0.1% henxol "/[ialcohol aud TUV/ wafer is eouieved hy a pipe 9i) lo the lreel slill Lllfmfever. il' a more roueeulraed alop is desired a l' ihe liol'loui oi'lhe heer Slilh ihe dilule alcohol from llze, pipe 91h instead olEheilig! comliufi'ed lo i'he column el, may be conveyed dii-eelhy a pipe100, lo he fusel oil discharge pipe l0, as Shown in Fig. Ahoelutealcohol is l'hua obtained in the column 72 and passes ouiA h v a ventedpipe lOl lo a disilling' kettle lllf' where the alcohol i5 vaporized h vineanS of a heating eoil 103 supplied with a current olz Steam. Thisvaporized alcohol passes up by a pipe 104i to a condenser 105 suppliedwith cooling wafer hav au. inlet pipe 10G and Uli aqlw- 1 Conta s il shit Vi LLL Weak u (th,

con

e i also ren ah 0b' Rahim W1 ,ein The um ww? my C to ohm h St m1 of h'l. a Waal f1 fanghi i man 'mfm U, LA.

hol and water, removing usel oil containing` alcohol during thedistillation ot the weal: alcohol and purifying` the fusel oil bydistillation and washing with water, 'the wash water being returned tothe tusel oil being distilled.

11. rlhe continuous process which coniprises distilling weak alcoholcontaining,

yateiand iinpurities containing tusel oil so as to obtain aqueous liquidalcohol ot' high strength containing usel oil, subjecting the alcohol ofhigh strength obtained therefrom to dehydration by distillation withathird liquid adapted to torni au az/.eotropic .ininture with thealcohol and water, removing tusel oil containing alcohol during' thedistillation ot the weak alcohol and purit'ying` the tusel oil bydistillation and washing with water, the wash water being returned tothe iusel oil being distilled.

l2. rllhe process Which comprises distilling weak alcohol newly suppliedto the process containing water so as to obtain aqueous liquid alcoholof high strength, subjecting the liquid alcohol oi high stren thobtained therefrom to dehydration by d...-tillatitni with a third liquidadapted to Ytorni au azeotropic mixture with the alcohol and water so asto obtain a distillate' forming separate. liquid layers, one containinga l lgher percentage ot alcohol than the othern and returning the layercontaining the higher percentage et alcohol a'liter the reinoral ot thethird liquid therelroiu, to the weak alcohol being distilled.

13. rlhe continuous process which coniprises distilling a weak alcoholnewly supplied to the process containing water so as to obtain aqueousliquid alcohol ot' high strengtln subjectiiug the. liquid alcohol othigh strength obtained theretroin to delirdration by distillation with athird liquid adapted to torni an azeotropic mixture with the. alcoholand water so as to obtain a distillati e iorniingseparate liquid layers`one coutaining a higher percentage ot alcohol than the other, andreturning` the layer coni aining the higher percentage ot alcohol utterthe renier-al oi the third liquid there trou: te the weak alcohol beingdistilled,

Ail. 'The process which comprises distilling` a wcal.; alcohol newlysupplied to the process containing water so as to obtain aqueous liquidalcohol ot high strength, subjecting the liquid alcohol ot high strengthobtained therefrom to dehydration by distillation with a third liquidadapted to forni an ancotropic mixture with the alcohol and water so asto obtain a distillate forming separate liquid layers. one containing ahigher percentage of alcohol and lower percentage otf the third liquidthan the other, returning the layer containing the higher percentage ofthird liquid to the high strength alcohol being dehydrated bydistillation and returning the layer containing the higher percentage otalcohol after the removal of the third liquid theret'roin, to the weakalcohol being distilled.

l5. rl`he continuous process which cornprises distilling a weak alcoholnewly supplied to the process containing water so as to obtain aqueousliquid alcohol ot high strength, subjecting the liquid alcohol of highstrength obtained there'troin to dehydration by distillation with athird liquid adapted to forni an azeotropic inixture with the alcoholand water so as to obtain a distillate *torining separate liquid layers,one containing a higher percentage ot alcohol and a lower percentage otthe third liquid than the other. returning the layer containing thehie'her percentage oll the third liquid tothe l i" istrength alcoholbeing dehydrated o v distillation and returning the layer containing'the higher percentage ot alcohol after the removal ot the third liquidtheretronr to be distilled with the weak alcohol.

lo. The process which comprises distilling` weak alcohol newly suppliedto the process containing water so as to obtain aqueous liquid alcoholot' high strength, subjecting the alcohol o'l high strength obtainedthere- 'troni to dehydration by distillation with a third liquid adaptedto torni an azeotropie mixture with the alcohol and water so to obtain adistillate 'forming separate liquid layers, one containing a higherpercentage otalcohol than the other. and returning the layer containingthe higher prccentage ol alcohol. atter haring passed through a washingopera tion` by means ol a material adapted to reinove. said thirdliquid, to the weak alcohol beingl distilled.

1T. The continuous process which coniprises dif-:tilling a weak alcoholnewly supplied to the prorei-is containing water so as to obtain aqueousliquid alcohol o't high strength` subjecting the alcohol ol highstrength obtained therefrom to dehydration by distillat ion with a thirdliquid adapted tol t'orin an azeotropic mixture with the alcohol andwater so as to obtain a distillate 'lornling separate. liquid layersI`one containing a higher percentage oit alcohol than the other, andreturning the layer containing the higher percentage ot' alcohol, afterharing passed through a washing operation by ineans of a. materialadapted to remove, said third liquid to the weak alcohol beingdistilled.

'18. The process which comprises distilling weak alcohol newly suppliedto the process containing' water so as to obtain aqueous liquid alcoholot high strength. subjecting the alcohol o't high strength obtainedtherefrom, while still warrn, to dehydration by distillation with athird liquid adapted to torni an azeotropic mixture with the alcohol andWater, and subjecting the dehydrated alc@4 to distillation to removesolid iiiipuiitie" therefrom.

19. The continuous process which con,n prises distilling Weel; alcoholnewly supplied to the process containing Weei' so us ic obtain aqueousliquid alcohol of high s45-length, subjecting the alcohol oi? highstrength oht-ained therefrom, While still wurm, to dehydration bydistillation with e. third liquid 10 adapted to form an ezeotropiciiiireure with Jche alcohol and Water, and subjecting the dehydratedalcohol to distillation to remove solid impurities hereiii'om.

ln. esimony that l claim the ioiegoing, l have hereunto set my hund this5 dey 0i May, i925.

EEWOUQ') l. CLLPP.

